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Designation: D1238 − 13

Standard Test Method for


Melt Flow Rates of Thermoplastics by Extrusion
Plastometer1
This standard is issued under the fixed designation D1238; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* Procedure C involves the use of a modified die, commonly


1.1 This test method covers the determination of the rate of referred to as a “half-die,” which has half the height and half
extrusion of molten thermoplastic resins using an extrusion the internal diameter of the standard die specified for use in
plastometer. After a specified preheating time, resin is extruded Procedures A and B thus maintaining the same length to
through a die with a specified length and orifice diameter under diameter ratio. The test procedure is similar to Procedure B, but
prescribed conditions of temperature, load, and piston position the results obtained with Procedure C shall not be assumed to
in the barrel. Four procedures are described. Comparable be half of those results produced with Procedure B.
results have been obtained by these procedures in interlabora- 1.5 Procedure D is a multi-weight test commonly referred to
tory round-robin measurements of several materials and are as a “Flow Rate Ratio” (FRR) test. Procedure D is designed to
described in Section 15. allow MFR determinations to be made using two or three
1.2 Procedure A is used to determine the melt flow rate different test loads (either increasing or decreasing the load
(MFR) of a thermoplastic material. The units of measure are during the test) on one charge of material. The FRR is a
grams of material/10 minutes (g/10 min). It is based on the dimensionless number derived by dividing the MFR at the
measurement of the mass of material that extrudes from the die higher test load by the MFR at the lower test load. Results
over a given period of time. It is generally used for materials generated from multi-weight tests shall not be directly com-
having melt flow rates that fall between 0.15 and 50 g/10 min pared with results derived from Procedure A or Procedure B.
NOTE 1—Polymers having melt flow rates less than 0.15 or greater than
(see Note 1). 900 g/10 min may be tested by the procedures in this test method;
1.3 Procedure B is an automatically timed measurement however, precision data have not been developed.
used to determine the melt flow rate (MFR) as well as the melt NOTE 2—Melt density is the density of the material in it molten state.
It is not to be confused with the standard density value of the material. See
volume rate (MVR) of thermoplastic materials. MFR measure- Table 3.
ments made with Procedure B are reported in g/10 minutes. NOTE 3—This test method and ISO 1133 address the same subject
MVR measurements are reported in cubic centimetres/ten matter, but differ in technical content.
minutes (cm3/10 min). Procedure B measurements are based 1.6 This standard does not purport to address the safety
on the determination of the volume of material extruded from concerns, if any, associated with its use. It is the responsibility
the die over a given period of time. The volume is converted to of the user of this standard to establish appropriate safety and
a mass measurement by multiplying the result by the melt health practices and determine the applicability of regulatory
density value for the material (see Note 2). Procedure B is limitations prior to use.
generally used with materials having melt flow rates from 0.50
to 1500 g/10 min. 2. Referenced Documents
1.4 Procedure C is an automatically timed measurement 2.1 ASTM Standards:2
used to determine the melt flow rate (MFR) of polyolefin D618 Practice for Conditioning Plastics for Testing
materials. It is generally used as an alternative to Procedure B D883 Terminology Relating to Plastics
on samples having melt flow rates greater than 75 g/10 min. D3364 Test Method for Flow Rates for Poly(Vinyl Chloride)
with Molecular Structural Implications
D4000 Classification System for Specifying Plastic Materi-
1
als
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.30 on Thermal Properties
2
(Section D20.30.08). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Aug. 1, 2013. Published August 2013. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1965. Last previous edition approved in 2010 as D1238 - 10. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D1238-13. the ASTM website.

*A Summary of Changes section appears at the end of this standard


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D1238 − 13
E691 Practice for Conducting an Interlaboratory Study to 5. Apparatus
Determine the Precision of a Test Method 5.1 Extrusion Plastometer (Alternative Names—Melt
2.2 ANSI Standard: Indexer, Melt Flow Indexer):
B46.1 on Surface Texture3
2.3 ISO Standard: NOTE 4—Older plastometers that were manufactured in accordance
with “design specifications” detailed in previous revisions of this test
ISO 1133 Determination of the Melt-Mass Flow Rate method (pre D1238 - 04c) are deemed to be acceptable, as long as they
(MFR) and the Melt Volume-Flow Rate (MVR) of Ther- meet the dimensional and performance specifications stated in this section.
moplastics3 NOTE 5—Relatively minor changes in the design and arrangement of
the component parts have been shown to cause differences in results
3. Terminology among laboratories. For the best interlaboratory agreement, it is important
that the design adhere closely to the description herein; otherwise, it
3.1 General: should be determined that modifications do not influence the results. Refer
3.1.1 Definitions are in accordance with Terminology D883 to Fig. 1.
unless otherwise specified.
5.1.1 The apparatus shall be a dead-weight piston plastome-
4. Significance and Use ter consisting of a thermostatically controlled heated steel
cylinder with a bore that contains a die at the lower end, and a
4.1 This test method is particularly useful for quality control
weighted piston operating within the cylinder. The essential
tests on thermoplastics.
features of the plastometer, illustrated in Figs. 1 and 2, are
4.2 The data produced by this test method serves to indicate described in 5.2-5.12. The bore of the extrusion plastometer
the uniformity of the flow rate of the polymer as made by an shall be properly aligned in the vertical direction (see Appen-
individual process. It is not to be used as an indication of dix X1). All dimensional measurements shall be made when
uniformity of other properties without valid correlation with the article being measured is at 23 6 5°C.
data from other tests.
5.2 Cylinder—The cylinder shall be 50 mm 6 10 mm in
4.3 The flow rate obtained with the extrusion plastometer is diameter, 115 to 180 mm in length with a smooth, straight bore
not a fundamental polymer property. It is an empirically 9.5504 6 0.0076 mm in diameter. The cylinder bore shall be
defined parameter critically influenced by the physical proper- manufactured in a way that produces a finish approximately 12
ties and molecular structure of the polymer and the conditions rms or better in accordance with ANSI B46.1. Means shall be
of measurement. The rheological characteristics of polymer provided to monitor the temperature inside the bore.
melts depend on a number of variables. It is possible that the
5.3 Die (Orifice):
values of these variables occurring in this test will differ
5.3.1 Standard Die—The outside diameter of the die shall
substantially from those in large-scale processes, which would
be such that it will fall freely to the bottom of the hole in the
result in data that does not correlate directly with processing
cylinder. The orifice of the die shall have a smooth straight bore
behavior.
2.095 6 0.005 mm in diameter and shall be 8.000 6 0.025 mm
4.4 Measure the flow rate of a material using any of the in length (see Fig. 2). The bore of the orifice and its finish are
conditions listed for the material in X4.1. For many materials, critical. It shall have no visible drill or other tool marks and no
there are specifications that require the use of this test method, detectable eccentricity. The bore of the orifice shall be manu-
but with some procedural modifications that take precedence factured by techniques known to produce finishes approxi-
when adhering to the specification. Therefore, it is advisable to mately 12 rms or better in accordance with ANSI B46.1.
refer to that material specification before using this test 5.3.2 “Half” Die—Used for Procedure C. When testing
method. Table 1 in Classification D4000 lists the ASTM polyolefins with a MFR of 75 or greater (using the standard
materials standards that currently exist. An alternative test die), an alternate die has shown to improve the reproducibility
method for poly (vinyl chloride) (PVC) compounds is found in of results by reducing the flow rate of these materials. The
Test Method D3364. outside diameter of the die shall be such that it will fall freely
4.5 Additional characterization of a material can be ob- to the bottom of the hole in the cylinder. The orifice shall have
tained if more than one condition is used. In the case that two a smooth straight bore 1.048 6 0.005 mm in diameter and shall
or more conditions are employed, a Flow Rate Ratio (FRR) is be 4.000 6 0.025 mm in length (see Fig. 2A). The bore of the
obtained by dividing the flow rate at one condition by the flow orifice and its finish are critical. It shall have no visible drill or
rate at another condition. Procedure D provides one method to other tool marks and no detectable eccentricity. The bore of the
measure more than one condition in a single charge. orifice shall be manufactured by techniques known to produce
finishes approximately 12 rms or better in accordance with
4.6 Frequently, variations in test technique, apparatus ANSI B46.1 (Note Note 6). No spacer shall be used with this
geometry, or test conditions, which defy all but the most die.
careful scrutiny, exist, causing discrepancies in flow rate NOTE 6—Recommended die material is tungsten carbide. Also satisfac-
determinations. A troubleshooting guide is found in Appendix tory are steel, synthetic sapphire, and cobalt-chromium-tungsten alloy.
X2 and it is a resource to be used to identify sources of test When softer materials are used, it will be necessary to conduct critical
error. dimensional checks and visual inspections on the die more often.
5.4 Piston:
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 5.4.1 The piston shall be made of steel. There shall be
4th Floor, New York, NY 10036, http://www.ansi.org. insulation at the top as a barrier to heat transfer from the piston

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D1238 − 13

FIG. 1 General Arrangement of Extrusion Plastometer (See Sec-


tion 5.)

FIG. 2 Details of Extrusion Plastometer

to the weight. The piston shall be prevented from rubbing on lower mark coincides with the top of the cylinder, guide sleeve
the bore. Most commercially available instruments use a loose or other suitable reference point, the bottom of the piston is 48
fitting metal guide sleeve, but other methods are acceptable. mm above the top of the die (see Fig. 1) and the timed test run
The weight of the sleeve shall not be considered as part of the shall start within these two reference marks. The targeted
test load. The land (foot) of the piston shall be starting point shall be 46 6 2mm above the upper face of the
9.4742 6 0.0076 mm in diameter and 6.35 6 0.10 mm in die. (see Fig. 1).
length. Above the land, the piston shall be relieved to ≤ 9.0 mm 5.4.3 The combined weight of piston and load shall be
in diameter (see Fig. 2). The piston land shall be manufactured within a tolerance of 60.5 % of the selected load.
by techniques known to produce finishes approximately 12 rms
in accordance with ANSI B46.1. If corrosion is a problem, the 5.5 Temperature Control System:
piston or piston land, if removable, shall be made of corrosion 5.5.1 The equipment shall have the capability of heating and
resistant material. maintaining the temperature inside the bore of the cylinder in
5.4.2 For procedure A, the piston shall be scribed with two accordance with the requirements specified in Table 1 through-
reference marks 4 mm apart in such fashion that when the out the duration of the test.

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D1238 − 13
TABLE 1 Maximum Allowable Variation in Temperature with between the piston tip and sidewall. Means of alignment are
Distance and Time Throughout the Test discussed in Appendix X1.
Test temperature Temperature tolerance, °C 5.7.2 Calibrated Go/No-Go Gauge:
set point
T °C At 75 ± 1 mm At 10 ± 1 mm
5.7.2.1 For the standard die, a go/no-go gauge suitable to
above the die above the die inspect the inner diameter of the hole in the die. The go
surface (°C)A surface (°C)A member of the gauge shall be no smaller than 2.090 mm. The
125 # T < 250 ±2.0 ±0.2
250 # T < 300 ±2.5 ±0.5 no-go member shall be no larger than 2.100 mm.
300 # T ±3.0 ±1.0 5.7.2.2 For the “half” die, a go/no-go gauge suitable to
A
When using the “half” die, the temperature indicating device shall be calibrated as inspect the hole in the die. The go member of the gauge shall
stated in this table except temperatures are measured at nominal 79 ± 1 mm and be no smaller than 1.043 mm. The no-go member shall be no
14 mm ± 1mm above the upper surface of the die.
larger than 1.053 mm.
5.7.3 Funnel—For charging samples to the cylinder
5.7.4 Packing Tool—For charging samples to the cylinder
5.5.2 The preferred method for calibrating the temperature 5.7.5 Spatula—Or similar device used to cut extrudate
is to use a temperature sensor assembly having a sensor with at 5.7.6 Balance—Capable of weighing to 0.001 g
least an accuracy of 60.08°C at 200°C and a 20 6 0.5-mm 5.8 Cleaning Equipment:
long brass tip press fit on the end of the sensor. The diameter 5.8.1 Cylinder bore cleaning tool
of the brass tip shall closely match the diameter of the die and 5.8.2 Die cleaning tool
the length of the active measuring length of the temperature 5.8.3 Cotton patches
sensor (see Appendix X3).
5.9 Weight Support—Used with high Melt Flow Rate mate-
5.5.3 Temperatures shall be verified with the bottom of the
rial to prevent material from flowing out during the preheat
temperature sensor at 10 and 75 6 1 mm above the upper face
period.
of the die and at each test temperature, without touching the
die. Allow at least four minutes for equilibrium of temperature 5.10 Die Plug—Used with high melt flow rate material to
to be reached for each position. Temperature variation shall be plug the die when weight support measures are not enough to
determined over a minimum of 15 minutes. When using the prevent material from flowing out during the preheat period.
“half” die, the temperature indicating device shall be calibrated 5.11 Automatic Weight Lowering and Lifting Device—
as stated in Table 1 except temperatures are measured at Optional for Procedures A, B, and C, but required for Proce-
79 6 1 mm and 14 6 1 mm above the upper surface of the die. dure D. Device for automatically applying test loads to the
5.5.4 An alternative method is to insert the temperature piston. This device is often useful as a weight support.
sensor without a brass tip into the melt from the top of the
cylinder so that it is 10 and 75 6 1 mm above the upper face 5.12 Multi-Weight (Flow Rate Ratio) Accessory—For test-
of the die. ing in accordance with Procedure D, it is necessary to have an
5.5.5 The temperature sensor and readout equipment used accessory that permits Melt Flow Rate determinations to be
for calibration of the extrusion plastometer shall be traceable to made using two or three different test loads on one charge of
a national standard (for example, NIST). material by loading or unloading test loads, or both, at pre-set
heights.
5.6 Timing Device/System—For Procedure A, a timing de- NOTE 7—Different manufacturers of equipment may offer options that
vice with an accuracy of 0.1 s shall be used. For Procedures B, help to automate the test and/or data collection. These are acceptable for
C, and D, an automatic timing system shall measure and time use provided they operate in a manner that does not conflict with
piston movement within the specified travel range. The re- descriptions in Section 5 and the procedures listed in Sections 9, 10, 11,
and 12.
quirements of the automatic timing system shall be as follows:
5.6.1 Sense and indicate the piston travel time within 60.01 6. Test Specimen
s.
5.6.2 Measure piston travel within 60.4 % of the nominal 6.1 The test specimen is permitted to be in any form that
selected value (see 10.7) for use in the flow rate calculations. allows it to be introduced into the bore of the cylinder, for
5.6.3 Operate within a fixed portion of the cylinder. This is example, powder, granules, strips of film, or molded slugs.
defined as the portion of the cylinder between 48 mm and NOTE 8—It may be desirable to pre-form or pelletize a powder. Trapped
18.35 mm above the top of the die. air causes the piston to fall faster, hence measurements are affected.
5.6.4 Any effects on the applied load caused by the Timing
Device/System must be included in the allowable tolerance 7. Conditioning
given in 5.4.3. 7.1 Many thermoplastic materials do not require condition-
5.6.5 The equipment used to calibrate the Timing Device/ ing prior to testing. Materials which contain volatile
System shall be traceable to a national standard (for example, components, are chemically reactive, or have other special
NIST). characteristics most probably require appropriate conditioning
5.7 Operating Tools: procedures. Moisture not only affects reproducibility of flow
5.7.1 Level—Used to verify the vertical alignment of the rate measurement but, in some types of materials, degradation
bore of the extrusion plastometer. This is necessary to mini- is accelerated by moisture at the high temperatures used in
mize subtractive loads resulting from rubbing or friction testing. Check the applicable material specification for any

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D1238 − 13
conditioning requirements before using this test. See Practice 9.6 Remove the piston from the bore (see Note 12). Within
D618 for appropriate conditioning practices. 60 seconds, charge the cylinder with a weighed portion of the
sample in accordance with the expected flow rate (as given in
8. Procedural Conditions Table 2), reinsert the piston and add the appropriate weight.
The charging weights given in Table 2 are merely suggestions,
8.1 A list of possible test conditions for various materials is
and the actual charging weight for a specific sample, if not
shown in Table X4.1 found in Appendix X4. Test conditions
known, will need to be determined by trial and error. Adjust the
shall be shown as: Condition _ _ _ / _ _ _, where the
charge weight so that the piston is in the proper position at the
temperature in degrees Celsius is shown first, followed by the
end of the pre-heat period. If necessary, it is acceptable to
weight in kilograms. For example: Condition 190/2.16.
purge excess material from the cylinder bore so that the piston
NOTE 9—Some materials may require special materials of construction is in the proper position at the end of the pre-heat period.
or handling for performing this test. Please refer to the material specifi- Purging of material done at conditions with greater force than
cation for appropriate recommendations.
testing conditions shall be completed at least 2 min prior to
making the initial cut-off (see Note 13).
9. Procedure A—Manual Operation
NOTE 12—Placing the piston on an insulated surface after removing it
9.1 Select conditions of temperature and load from X4.1 or from the bore will reduce heat loss.
in accordance with material specifications. Where multiple test NOTE 13—Material is purged by forcing the piston to a position that
conditions exist, test conditions shall be agreed upon by the will ensure that subsequent travel of the piston during the remainder of the
cooperating laboratories. If test conditions are not known, pre-heat period will position the piston at the correct start position. The
material should be allowed to soften and melt before manually purging.
select conditions that result in flow rates between 0.15 to 50 NOTE 14—Additional care may be necessary to prevent thermal
g/10 min. degradation in the extrusion plastometer. This is sometimes done by the
9.2 Inspect the extrusion plastometer for cleanliness (see addition of an appropriate antioxidant. For highly unstable materials, it
may be necessary to use alternative techniques as an indication of flow
Note 10). All surfaces of the cylinder bore, die and piston shall characteristics.
be free of any residue from previous tests.
9.7 Start the test by initiating the timing device that moni-
NOTE 10—The degree of cleanliness can significantly influence the flow tors the pre-heat period, which is a period of time that allows
rate results, therefore a thorough method of cleaning should be estab- the material to soften and begin to melt. The pre-heat period
lished. It has been found that swabbing the barrel with a clean cotton patch
several times is satisfactory for most materials and that the die, barrel, and
shall last for 7.0 6 0.5 min from the completion of the charge
piston are more easily cleaned while hot. For materials that are difficult to unless otherwise stated in the materials specification.
clean from the metal surfaces, use of a brass brush has been found to be 9.8 For materials with flow rates greater than 10 g/10 min,
satisfactory.
a weight (and if needed, a piston) support must be used to
9.3 Check the die bore diameter at frequent intervals with prevent the piston from travelling during the pre-heat period in
appropriately sized go/no-go gauges (checked with die at order to ensure that there is enough material in the bore to
23 6 5°C) to verify that the die is within the tolerances given correctly test the material. The support is to be installed in a
in 5.3.1. Visually examine the die bore to verify that it is not
scratched or damaged. Also visually inspect the land of the
piston foot to verify that it is not scratched or damaged and use TABLE 2 Standard Test Conditions, Sample Mass,A and Testing
a calibrated micrometer to verify that the dimensions are within TimeB
the tolerances given in 5.4.1 (see Note 11). Suggested Mass
Factor for
Flow Range, of Time Inter-
Obtaining Flow
NOTE 11—Cleaning and usage will eventually cause damage or wear to g/10 min Sample in val, min
Rate in g/10 min
Cylinder, g
the, bore, die and the land of the piston. Data has shown that erroneous
results will be obtained if these components are not within the appropriate 0.15 to 1.0 2.5 to 3.0 6.00 1.67
tolerances. >1.0 to 3.5 3.0 to 5.0 3.00 3.33
>3.5 to 10 4.0 to 8.0 1.00 10.00
9.4 Set the temperature in accordance with the manufactur- >10 to 25 4.0 to 8.0 0.50 20.00
>25 4.0 to 8.0 0.25 40.00
er’s instructions.
A
This is a suggested mass for materials with melt densities of about 0.7 g/cm3.
9.5 Insert the die and the piston into the bore. Allow the Correspondingly, greater quantities are suggested for materials of greater melt
temperature of the cylinder, with the piston and die in place, to densities. Density of the molten resin (without filler) may be obtained using the
procedure described by Terry, B. W., and Yang, K., “A New Method for Determining
stabilize within 60.2°C of the selected test temperature for at Melt Density as a Function of Pressure and Temperature,” SPE Journal , SPEJA,
least 15 min before starting a test. When equipment is used Vol. 20, No. 6, June 1964, p. 540 or the procedure described by Zoller, Paul, “The
continuously, it is not necessary to heat the piston and die for Pressure-Volume-Temperature Properties of Polyolefins,”Journal of Applied Poly-
mer Science, Vol 23, 1979, p. 1051. It may also be obtained from the weight of an
15 minutes when runs of the same or similar material at the extruded known volume of resin at the desired temperature. For example, 25.4 mm
same test temperature are being measured over a continuous (1 in.) of piston movement extrudes 1.804 cm3 of resin. An estimate of the density
time frame, provided the piston and die are cleaned and of the material can be calculated from the following equation:

re-inserted into the bore within five minutes after removal from resin density at test temperature 5 M/1.804
the extrusion plastometer at the end of each test. If the piston, where:
or die, or both, are removed from the bore for longer than five M = mass of extruded resin.
minutes, they shall be considered “cold” and the full 15 B
See 9.13.
minutes heating stabilization time shall be required.

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D1238 − 13
manner that holds the lower scribe mark of the piston approxi- 10. Procedure B—Automatically Timed Flow Rate
mately 25 mm above the top of the guide bushing or other Measurement
suitable reference mark. Alternatively, it is acceptable for the 10.1 Install/enable the automatic timing device on the ex-
operator to delay applying the weight to the piston. The support trusion plastometer.
shall be removed or the weight applied to the piston at such a
time as to allow the operator to make the initial cut-off within 10.2 Select conditions of temperature and load from Table
7 6 0.5 min of the completion of the charge. X4.1 or in accordance with material specifications. Where
multiple test conditions exist, test conditions shall be agreed
NOTE 15—It has been found that the effect of supporting the weight is upon by the cooperating laboratories. A melt density value (see
significant to the flow rate results. The choice of piston support was made Table 2 and Table 3) for the material is required if MFR is to
to cover all conditions and flow rates 10 to 50 g/10 min. Piston/weight be calculated from the results.
supports will vary between extrusion plastometer manufacturers.
10.3 Inspect the extrusion plastometer for cleanliness (see
9.9 At the end of the pre-heat period and when the top scribe Note 17). All surfaces of the cylinder bore, die and piston shall
mark on the piston is visible above the cylinder (or top of the be free of any residue from previous tests.
guide sleeve) and the lower scribe mark is in the cylinder (or
below the top of the guide sleeve) indicating that the piston 10.4 Check the die bore diameter at frequent intervals with
land is 46 6 2 mm from the top of the die, reset the timer to appropriately sized go/no-go gauges (checked with die at
zero then simultaneously make the initial cut-off. Discard the 23 6 5°C) to verify that the die is within the tolerances given
extrudate from the pre-heat period. Make the final cut-off in 5.3. Visually examine the die bore to verify that it is not
exactly when the time interval selected (see Table 2) is reached. scratched or damaged. Also visually inspect the land of the
Collect and weigh the extrudate specimen. If the extrudate piston foot to verify that it is not scratched or damaged and use
specimen contains visible bubbles, discard it and begin the test a calibrated micrometer to verify that the dimensions are within
again. If the initial cut-off was initiated outside of the toler- the tolerances given in 5.4.1 (see Note 11).
ances of the pre-heat period or the piston position 10.5 Set the temperature in accordance with the manufac-
requirements, discard the specimen and repeat the test with turer’s instructions.
readjusted piston position after the initial purge, or change the 10.6 Insert the die and the piston into the bore. Allow the
weight. temperature of the cylinder with the piston and die in place to
9.10 Once the extrudate is cool, weigh to the nearest 1 mg. stabilize within 60.2°C of the selected test temperature for at
least 15 min before starting a test. When equipment is used
9.11 Multiply the weight of the extrudate by the appropriate continuously, it is not necessary to heat the piston and die for
factor shown in Table 2 to obtain the flow rate in grams per 10 15 minutes when runs of the same or similar material at the
min. same test temperature are being measured over a continuous
time frame, provided the piston and die are cleaned and
NOTE 16—Some labs have found it helpful to take interim cuts of the
extrudate at uniform time intervals during the specified extrusion time re-inserted into the bore within five minutes after removal from
period. The individual cuts may give an indication of the presence of the extrusion plastometer at the end of each test. If the piston,
bubbles which may be masked due to their size or to opacity of the sample or die, or both, are removed from the bore for longer than five
which will result in test error. This technique is particularly helpful in the minutes, they shall be considered “cold” and the full 15
case of highly pigmented materials. minutes heating stabilization time shall be required.
9.12 Purge the remainder of the sample from the bore and 10.7 Adjust the automatic timing system to operate within
follow the extrusion plastometer manufacturer’s instructions the 6.35 6 0.25 mm measuring range for materials with
for removing the die from the bore. Swab out the cylinder with expected melt flow rates of up to 10 g/10 min, or 25.40 6 0.25
cotton patches and the cylinder bore cleaning tool. Thoroughly mm measuring range for materials with expected melt flow
clean the die and the piston to remove all residues (Note Note
17).
NOTE 17—The die may be cleaned by dissolving the residue in a
solvent. A better method is pyrolytic decomposition of the residue in a TABLE 3 Factors for Calculation of Flow Rate
nitrogen atmosphere. Place the die in a tubular combustion furnace or Factor for
other device for heating to 550 6 10°C and clean with a small nitrogen Material Tempera- Piston Travel, Calculation of
purge through the die. This method is preferable to flame or solvent (Unpigmented) ture, °C L, cm (in.) Flow
cleaning, being faster than solvent cleaning and less detrimental to the die Rate, FA
than an open flame. In certain cases where materials of a given class Polyethylene 190 2.54 (1) 826
having similar flow characteristics are being tested consecutively, interim Polyethylene 190 0.635 (0.25) 207
die cleaning may be unnecessary. In such cases, however, the effect of Polypropylene 230 2.54 (1) 799
cleaning upon flow rate determination must be shown to be negligible if Polypropylene 230 0.635 (0.25) 200
this step is avoided. A
Factors calculated using melt-density values of 0.7636 g/cm3 for polyethylene
and 0.7386 g/cm3 for polypropylene, as expressed in article by Zoller, Paul, “The
9.13 In case a specimen has a flow rate at the borderline of Pressure-Volume-Temperature Properties of Polyolefins,” Journal of Applied Poly-
the ranges in Table 2 and slightly different values are obtained mer Science, Vol 23, 1979, P. 1051. The base densities at 23°C for which the melt
densities are reported were 0.917 g/dm3 for annealed low-density polyethylene
at different time intervals, the referee value shall be obtained at and polypropylene homopolymer.
the longer time interval.

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rates of 10 g/10 min or higher and set to begin timing when the 10.13 Record the time to the nearest 0.01 s for the piston to
bottom of the piston foot is 46 6 2 mm above the top of the complete the selected distance of travel.
die. 10.14 Purge the remainder of the sample from the bore and
NOTE 18—It has been found that for some materials the melt flow rates follow the extrusion plastometer manufacturer’s instructions
obtained on a material will be different depending on which travel length for removing the die from the bore. Swab out the cylinder with
is chosen; therefore, it is important to use the same measurement range to cotton patches and the cylinder bore cleaning tool. Thoroughly
compare interlaboratory results.
clean the die and the piston to remove all residues (see Note
10.8 Remove the piston from the bore (see Note 12). Within 10).
60 seconds, charge the cylinder with a weighed portion of the
sample in accordance with the expected flow rate (as given in 11. Procedure C— Automatically Timed Flow Rate
Table 2), reinsert the piston and add the appropriate weight. Measurement for High Flow Rate Polyolefins Using
The charging weights given in Table 2 are merely suggestions, “Half” Die
and the actual charging weight for a specific sample, if not 11.1 Procedure:
known, will need to be determined by trial and error. Adjust the 11.1.1 Install/enable the automatic timing device on the
charge weight so that the piston is in the proper position at the extrusion plastometer.
end of the pre-heat period. If necessary, it is acceptable to 11.1.2 Select conditions of temperature and load from X4.1
purge excess material from the cylinder bore so that the piston or in accordance with material specifications. Where multiple
is in the proper position at the end of the pre-heat period. test conditions exist, test conditions shall be agreed upon by the
Purging of material done at conditions with greater force than cooperating laboratories. A melt density value (not bulk den-
testing conditions shall be completed at least 2 min prior to the sity) for the material is required if MFR is to be calculated from
expiration of the preheat period (see Note 13). the results.
10.9 Start the test by initiating the timing device that 11.1.3 Use the procedure described in 10.3 – 10.14with the
monitors the pre-heat period, which is a period of time that following exceptions:
allows the material to soften and begin to melt. The pre-heat 11.1.3.1 Use the “half” die as described in 5.3.2.
period shall last for 7.0 6 0.5 min from the completion of the 11.1.3.2 Adjust the timing device to operate within the
charge unless otherwise stated in the materials specification. 25.40 6 0.25 mm measuring range and set to begin timing
when the bottom of the piston foot is 50 6 2 mm above the top
10.10 For materials with flow rates greater than 10 g/10 of the die.
min, a weight (and if needed, a piston) support must be used to
prevent the piston from travelling during the pre-heat period in 12. Procedure D—Multi-Weight Using Automatically
order to ensure that there is enough material in the bore to Timed Flow Rate Measurement
correctly test the material. The support is to be installed in a 12.1 Procedure:
manner that holds the lower scribe mark of the piston approxi- 12.1.1 Install/enable the automatic timing device, automatic
mately 25 mm above the top of the guide bushing or other weight lifting/lowering device and multi-weight (FRR) acces-
suitable reference mark. Alternatively, it is acceptable for the sory on the extrusion plastometer. The multi-weight test shall
operator to delay applying the weight to the piston. The support be made in either increasing weight or decreasing weight
shall be removed or the weight applied to the piston at such a conditions. Follow the equipment manufacturer’s instructions
time as to allow the measurement to start within 7 6 0.5 min of for installation and operation.
the completion of the charge. (For automated weight lowering 12.1.2 Configure the multi-weight (FRR) accessory to take
systems, the bottom of the piston foot is held at approximately at least two MFR determinations at each load condition used
71 mm above the top of the die.) before changing to the next test load. After switching load
10.11 For materials greater than 50 g/10 min, use of a die conditions, achieve stable flow by allowing sufficient piston
plug is an option in addition to the piston/weight support. The travel or time to elapse before beginning measurements (see
die plug is inserted before charge and is removed prior to Note 19). Piston travel distances shall be chosen so that at least
removing the piston/weight support. (Warning—Rapid expul- 2 seconds elapse during the measurement and that the distances
sion of material when die plug is removed is hazardous.) are determined within 60.4 %.
10.12 At the end of the pre-heat period and when automatic NOTE 19—Normally, 5 mm of piston travel or 2 min is sufficient to
timing system senses that the piston has reached the pre- obtain stable flow after changing test loads.
selected starting point (indicating that the piston land is 46 6 2 12.1.3 Adjust the automatic timing device to make multiple
mm from the top of the die), the automatic timing system shall test measurements as required and set to begin timing the first
begin measuring the time it takes for the piston to travel the measurement when the bottom of the piston foot is 46 6 2 mm
pre-selected distance (see 10.7). If the extrudate specimen above the top of the die. Do not take readings below 18.35 mm
contains visible bubbles, discard the results and begin the test above the top of the die.
again (see Note 13). If the initial timed measurement was 12.1.4 Inspect the extrusion plastometer for cleanliness (see
initiated outside of the tolerances of the pre-heat period or the Note 10). All surfaces of the cylinder bore, die and piston shall
piston position requirements, discard the results and repeat the be free of any residue from previous tests.
test after readjusting the piston position after the initial purge 12.1.5 Check the die bore diameter at frequent intervals
or changing the charge weight. with appropriately sized go/no-go gauges (checked with die at

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23 6 5°C) to verify that the die is within the tolerances given 12.1.13 Record the time, to the nearest 0.01 s, for the
in 5.3.1. Visually examine the die bore to verify that it is not individual piston travel determinations measured for each test
scratched or damaged. Also visually inspect the land of the load.
piston foot to verify that it is not scratched or damaged and use 12.1.14 Repeat the above for any additional test loads.
a calibrated micrometer to verify that the dimensions are within 12.1.15 Purge the remainder of the sample from the bore
the tolerances given in 5.4.1 (see Note 11). and follow the extrusion plastometer manufacturer’s instruc-
12.1.6 Set the temperature in accordance with the manufac- tions for removing the die from the bore. Swab out the cylinder
turer’s instructions. with cotton patches and the cylinder bore cleaning tool.
Thoroughly clean the die and the piston to remove all residues
12.1.7 A melt density value (see Table 2) for the material is
(see Note 10).
required in order to calculate MFR for the individual determi-
nations.
13. Calculation of Flow Rate
12.1.8 Insert the die and the piston into the bore. Allow the
temperature of the cylinder with the piston and die in place to 13.1 Calculation for Procedures B and C:
stabilize within 60.2°C of the selected test temperature for at 13.1.1 Calculate the flow rate in grams per 10 min or
least 15 min before starting a test. When equipment is used volume rate in cm3 per 10 min as follows (see Note 20):
continuously, it is not necessary to heat the piston and die for Melt flow rate 5 ~ 426 3 L 3 d ! /t
15 minutes when runs of the same or similar material at the or
same test temperature are being measured over a continuous Melt volume rate 5 426 3 L/t
time frame, provided the piston and die are cleaned and
re-inserted into the bore within five minutes after removal from where:
the extrusion plastometer at the end of each test. If the piston L = length, cm, of calibrated piston travel,
and/or die are removed from the bore for longer than five d = melt density of resin, g/cm3, at test temperature, (see
minutes, they shall be considered “cold” and the full 15 reference under Table 2 and Table 3),
t = time, seconds, of piston travel for length L, and
minutes heating stabilization time shall be required.
426 = mean of areas, cm2, of piston and cylinder × 600.
12.1.9 Remove the piston from the bore (see Note 12). NOTE 20—Factors that may be substituted in the following equation are
Within 60 seconds, charge the cylinder with a weighed portion given for some materials in Table 3.
of the sample in accordance with the expected melt flow rate
Flow rate, g/10min 5 F/t
(as given in Table 2), reinsert the piston and use the weight
lifting and lowering device to add the test load to the piston. where:
12.1.10 Some materials, particularly those with expected F = factor from Table 3, and
melt flow rates less than 10g/10 min during the first measure- t = time, seconds, of piston travel for length L.
ment period require the operator to purge some material to a 13.1.2 Improved agreement between Procedures A and au-
position that insures subsequent travel of the piston will tomatically timed flow measurements (Procedures B, C, and D)
activate the timing device at the desired starting point for the is obtained if an average melt density for a particular type of
first measurement within 7.0 6 0.5 min after the completion of material is determined with the actual equipment used and that
the charge. The lower scribe mark of the piston shall be at least value is substituted into the equation given in 13.1.1.
25 mm above the top of the cylinder after purging. Any purging
must be completed at least 2 min prior to start of the test Melt 13.2 Calculation for Procedure D:
Flow Rates. 13.2.1 Calculate the MFR for each capture at each test load
in accordance with Section 10 (Procedure B).
12.1.11 Materials with higher expected flow rates will
13.2.2 If the differences between the individual melt flow
require that the weight and piston support be used after
rates at each test load are no greater than 63 %, calculate the
charging the material. For Procedure D, this can be accom-
average Melt Flow Rate for each test load. If differences are >
plished with the automatic weight lifting/lowering device. The 63 % repeat the test.
support shall be removed at such a time as to allow the
automatic timing device to activate at the starting point for the NOTE 21—To achieve stable flow after applying each test load, it may
first measurement within 7.0 6 0.5 min after the completion of be necessary to increase the time or the piston travel distance before taking
a measurement.
the charge. Only use the piston support if there is excessive
material flow (see Note 15). 13.2.3 Calculate the Flow Rate Ratio (FRR) as the ratio of
12.1.12 If a die plug is used to prevent excessive leakage the average flow rate at the higher load to the average flow rate
before the test, for materials with a melt flow rate greater than at the lower load.
50 g/10 min, then the die plug is to be inserted before the
charge and removed prior to removing the piston/weight 14. Report
support. The initial charge shall be adjusted to ensure appro- 14.1 Report the following information:
priate measurement loads based on suggestions in Table 2. If 14.1.1 Statement indicating the nature and physical form of
the timer is not activated within 7 6 0.5 min after the the material charged to the cylinder.
completion of the charge the test must be repeated with 14.1.2 Temperature and load at which the test is run shall be
readjusted charge weights. reported. The results and test conditions, along with an

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TABLE 4 Precision, Procedure A (Values in g/10 min)
Number of
Material Condition Average SrA SRB IrC IRD
Laboratories
Polyethylene 190/2.16 0.27 0.008 0.022 0.023 0.063 9
Polyethylene 190/2.16 0.40 0.012 0.038 0.035 0.108 9
Polyethylene 190/2.16 2.04 0.026 0.079 0.073 0.224 9
Polyethylene 190/2.16 44.1 0.919 1.232 2.560 3.486 7
Polypropylene 230/2.16 2.23 0.106 0.226 0.299 0.639 9
Polypropylene 230/2.16 7.09 0.222 0.471 0.627 1.331 9
Polypropylene 230/2.16 32.8 0.581 1.051 1.644 2.974 9
Polystyrene 200/5 1.67 0.024 0.122 0.068 0.344 6
Polystyrene 200/5 8.82 0.190 0.667 0.538 1.886 6
Polystyrene 200/5 13.3 0.305 0.925 0.864 2.617 6
Polycarbonate 300/1.2 2.41 0.076 0.115 0.215 0.326 4
Polycarbonate 300/1.2 10.5 0.429 0.647 1.215 1.830 4
Polycarbonate 300/1.2 16.2 0.155 1.109 0.438 3.140 4
Acrylic 230/3.8 2.59 0.051 0.051 0.145 0.145 3
A
S r = within-laboratory standard deviation of the average.
B
SR = between-laboratories standard deviation of the average.
C
Ir = 2.83Sr, and
D
IR =2.83 S R.

TABLE 5 Precision, Procedure B (Values in g/10 min)


Number of
Material Condition Average SrA SRB IrC IRD
Laboratories
Polyethylene 190/2.16 0.27 0.009 0.014 0.026 0.039 8
Polyethylene 190/2.16 0.40 0.016 0.027 0.045 0.076 8
Polyethylene 190/2.16 2.04 0.040 0.094 0.112 0.266 9
Polyethylene 190/2.16 43.7 0.997 1.924 2.819 5.443 8
Polypropylene 230/2.16 2.25 0.052 0.214 0.1466 0.604 8
Polypropylene 230/2.16 7.16 0.143 0.589 0.4051 1.666 8
Polypropylene 230/2.16 32.6 0.693 0.945 1.959 2.672 8
Polystyrene 200/5 1.65 0.037 0.166 0.106 0.470 4
Polystyrene 200/5 8.39 0.144 0.423 0.406 1.197 4
Polystyrene 200/5 13.0 0.108 0.387 0.306 1.097 4
A
S r = within-laboratory standard deviation of the average.
B
SR = between-laboratories standard deviation of the average.
C
Ir = 2.83Sr, and
D
IR= 2.83SR.

TABLE 6 Precision, Procedure A (Values in g/10 min)


Number of
Material Condition Average SrA SRB rC RD
Labs
Acrylic 230/3.8 1.51 0.013 0.086 0.037 0.242 7
LDPE 190/2.16 1.74 0.027 0.052 0.075 0.144 11
Polystyrene 200/5.0 1.86 0.040 0.085 0.112 0.238 9
HDPE 190/2.16 5.35 0.049 0.103 0.137 0.288 11
Polypropylene 230/2.16 10.94 0.088 0.473 0.247 1.324 10
Polycarbonate 300/1.2 13.59 0.109 0.233 0.305 0.653 4E
Acetal 190/2.16 25.30 0.235 0.571 0.658 1.599 7
A
S r = within-laboratory standard deviation of the average.
B
SR = between-laboratories standard deviation of the average.
C
r =2.83Sr.
D
R = 2.83SR .
E
Insufficient laboratories to meet Practice E691.

indication of which procedure was used (for example, Proce- 14.1.4 Procedure used (A, B, C, or D).
dure C-190/2.16) shall be documented. Reference shall be 14.1.5 Any unusual behavior of the test specimen such as
made to this test method. discoloration, sticking, extrudate surface irregularity or
NOTE 22—It has become customary to refer to the flow rate of
roughness, etc.
polyethylene as “melt index” when obtained under Condition 190/2.16. 14.1.6 Details of conditioning, if any.
However, for all other materials the use of melt index or any term other 14.1.7 For multi-weight tests using Procedure D, also re-
than “melt flow rate” is discouraged, regardless of the condition used. port:
14.1.3 Melt flow rate reported as the rate of extrusion in 14.1.7.1 The average flow rate at each test load.
grams per 10 min or volume rate in cm3 per 10 min. Data 14.1.7.2 The Flow Rate Ratio (FRR) together with the
should be reported to three significant figures. temperature and loads used (for example, FRR-190/21.6/2.16).

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TABLE 7 Precision, Procedure B (Values in g/10 min)
Number of
Material Condition Average SrA SRB rC RD
Labs
Acrylic 230/3.8 1.54 0.026 0.102 0.072 0.286 6
LDPE 190/2.16 1.76 0.015 0.053 0.042 0.149 11
Polystyrene 200/5.0 1.89 0.042 0.102 0.117 0.285 7
HDPE 190/2.16 5.41 0.041 0.113 0.114 0.316 10
Polypropylene 230/2.16 10.96 0.357 0.491 0.999 1.376 10
Polycarbonate 300/1.2 13.79 0.104 0.477 0.292 1.335 3E
Acetal 190/2.16 25.64 0.182 0.822 0.508 2.302 6
A
S r = within-laboratory standard deviation of the average.
B
SR = between-laboratories standard deviation of the average.
C
r = 2.83Sr.
D
R = 2.83SR.
E
Insufficient laboratories to meet Practice E691.

TABLE 8 Precision, Procedure B (Values in g/10 min) should apply the principles outlined in Practice E691 to
Material Condition Average SrA SRB IrC IRD generate data specific to their laboratory and materials. The
Polypropylene 230/2.16 245 13.2 16.6 37.4 46.9 principles of 15.1.4 – 15.1.7 would then be valid for such data.)
Polypropylene 230/2.16 482 31.8 40.0 89.9 113 15.1.3 Table 9 is based on a round robin conducted in 1999
Polypropylene 230/2.16 837 20.9 58.6 59.1 166
Polypropylene 230/2.16 1603 129 243 365 688 on Procedure C. Data for seven of the eight participating
A
S r = within-laboratory standard deviation of the average.
laboratories were included in the statistics for this table. Four
B
SR = between-laboratories standard deviation of the average. polyethylene materials were tested with melt flow rates using
C
D
Ir= 2.83Sr, and the standard die ranging from approximately 35 to 2350 g/10
IR= 2.83SR.
min using the “half-die” die.
15.1.4 Concept of Ir and IR—Relevant if Sr and SR have
been calculated from a large enough body of data, and if test
14.1.7.3 Whether the decreasing or increasing load tech- results are averages obtained from testing two specimens.
nique was used. 15.1.5 Repeatability, Ir—In comparing two test results for
the same material, obtained by the same operator using the
15. Precision and Bias (Procedures A, B, and C) same equipment on the same day, judge the two test results as
15.1 Precision: not equivalent if they differ by more than the Ir value for that
15.1.1 Tables 4 and 5 are based on a round robin4 conducted material.
in 1986 and 1987, involving polypropylene, polyethylene, 15.1.6 Reproducibility, IR—In comparing two test results for
polystyrene, polycarbonate and acrylic materials. Tables 6 and the same material, obtained by different operators using differ-
7 are based on a round robin5 completed in 1997 involving low ent equipment on different days, judge the two test results as
and high density polyethylene, polypropylene, polystyrene, not equivalent if they differ by more than the IR value for that
polycarbonate, PMMA, and acetal. The number of participat- material.
ing laboratories is shown for each material. Data for Tables 4 15.1.7 Any judgment in accordance with 15.1.4 and 15.1.6
and 5 were generated through each lab testing two specimens would have an approximate 95 % (0.95) probability of being
for each material on three different days, while data for Tables correct.
6 and 7 were generated through each lab testing two specimens 15.2 Bias—There are no recognized standards by which to
for each material on two different days. The analysis in Practice estimate bias of this test method.
E691 is based on a test result being the average of two
specimens. 16. Precision and Bias (Procedure D)
15.1.2 Table 8 is based on a round robin6 conducted in 1980
using Procedure B. Four polypropylene samples having flow 16.1 Precision
rates from 250 to 1500 were tested in nine laboratories. 16.1.1 Procedure D used as many as nine laboratories, five
(Warning—The following explanations of Ir and IR (15.1.4 – materials and two determinations in order to come up with the
15.1.6) are only intended to present a meaningful way of
considering the approximate precision of this test method. The
data in Tables 4-8 should not be vigorously applied to TABLE 9 Precision Data for High Melt Flow Polyolefins
Procedure C (Values in g/10 min)A
acceptance or rejection of material since those data are specific
MaterialsB Average Sr SR r R
to the round robin and may not be representative of other lots, PE-A (35) 4.67 0.068 0.119 0.191 0.334
conditions, materials or laboratories. Users of this test method PE-B (185) 24.30 0.688 1.168 1.928 3.270
PE-C (2350) 315.7 10.81 19.89 30.27 55.69
PE-D (122) 16.20 0.188 0.348 0.526 0.975
4
Supporting data are available from ASTM Headquarters. Request RR:D20- A
This data was generated with dies having a nominal length of 3.985 mm versus
1164. the required 4.000 mm.
5
Supporting data are available from ASTM Headquarters. B
Numbers in parentheses are approximate melt flow rate values of materials using
6
Supporting data are available from ASTM Headquarters. Request RR:D20- standard die (5.3).
1124.

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following tables of precision supporting the method. This TABLE 12 Precision Statement for Procedure D: 10 kg
meets or exceeds all the standards required for Practice E691. Materials Average Sr SR r R
16.1.2 The degree of precision is quite high for all levels of PE1 11.6841 0.3065 0.4595 0.8581 1.2867
PE2 7.5768 0.1266 0.2751 0.3544 0.7704
loads on the ram. The highest level of precision was attained PE3 4.1181 0.0535 0.1036 0.1497 0.2902
for the 2.16 kg load, the lowest for the 21.6 kg load. It is PE4 3.7693 0.0538 0.1125 0.1507 0.3151
important to note that the 21.6 kg load is not optimum for the PE5 3.3471 0.0228 0.0647 0.0638 0.1812

standard (8.00 mm) die because the speed of testing does not TABLE 13 Precision Statement for Procedure D: 21.6 kg
allow for the flow to reach probably equilibrium rate. Refer to Materials Average Sr SR r R
PE1 59.9335 2.1012 2.7667 5.8833 7.7469
Table 10 for 2.16 kg load; Table 11 for 5 kg load; Table 12 for PE2 36.2367 1.4450 1.4450 4.0459 4.0459
10 kg load and Table 13 for 21.6 kg load. PE3 14.1078 0.1662 0.3352 0.4653 0.9387
TABLE 10 Precision Statement for Procedure D: 2.16 kg PE4 17.6132 0.3324 0.4258 0.9308 1.1924
PE5 12.2652 0.1104 0.4590 0.3090 1.2851
Materials Average Sr SR r R
PE1 0.7567 0.0079 0.0323 0.0220 0.0904
PE2 0.4298 0.0060 0.0277 0.0168 0.0776 17. Keywords
PE3 0.5527 0.0096 0.0179 0.0268 0.0502
PE4 0.2627 0.0043 0.0182 0.0120 0.0511 17.1 melt flow rate; melt index; volume flow rate
PE5 0.4104 0.0079 0.0119 0.0222 0.0334
TABLE 11 Precision Statement for Procedure D: 5 kg
Materials Average Sr SR r R
PE1 3.0561 0.7715 0.7809 2.1602 2.1865
PE2 1.9960 0.0483 0.0927 0.1353 0.2595
PE3 1.5821 0.0260 0.0462 0.0729 0.1293
PE4 0.9976 0.2158 0.2560 0.6042 0.7168
PE5 1.2308 0.0170 0.0285 0.0475 0.0798

APPENDIXES

(Nonmandatory Information)

X1. EXTRUSION PLASTOMETER BORE ALIGNMENT

X1.1 A fixture consisting of a circular level mounted on a insertion into the bore may also be satisfactory. A circular level
shaft having two bearing points 9.48 6 0.01 mm in diameter having a sensitivity of 20 min/2.5 mm has been found
that can be inserted into the bore has been found suitable. A satisfactory. Other alignment techniques that give comparable
circular level that can be rigidly mounted on the piston rod for alignment sensitivity would be considered satisfactory.

X2. TROUBLESHOOTING GUIDE

INTRODUCTION

This appendix is offered in an effort to help a laboratory improve melt flow rate testing and to get
to the root cause of problems which may be caused by equipment, environment, or testing technique.
This guide is not meant to be an all-inclusive trouble-shooting check list, but merely tries to help users
to evaluate testing to some degree.

X2.1 Basic Programs SRM 1474 with a flow rate of 5.03 g/10 min, SRM 1496 with a flow rate
of 0.26 g/10 min, and SRM 1497 with a flow rate of 0.19 g/10 min. SRM
X2.1.1 The following are basic programs in which all 1475a is certified under condition 190/3.25 with a flow rate of 2.20 g/10
laboratories should participate: min.7
X2.1.1.1 Standard Reference Materials—If available, SRMs X2.1.1.2 Internal Controls—An internal control for each
can usually be obtained from a national metrological institute type of material should be set up. This involves setting aside
(for example, National Institute of Standards and Technology). enough material to last a long time (at least one year). These
These SRMs provide accurate information on the melt flow materials will have to be tested many times to establish
rate of these materials. However, these SRMs are expensive statistical parameters. Each time an internal standard is run, the
and are available for a very limited number of materials.
NOTE X2.1—Satisfactory operation of the apparatus for polyethylenes
can be ascertained by making measurements on NIST Standard Reference 7
These standard polyethylenes are available from the National Institute of
Materials (SRMs) certified for melt flow rate. The four SRMs certified Standards and Technology, Office of Standard Reference Materials, Washington, DC
under condition 190/2.16 are SRM 1473 with a flow rate of 1.29 g/min, 20234.

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results should be plotted on a SQC chart so that any problems may also scratch the barrel. The piston must move in an exact
or trends can be detected quickly. A SQC chart should be set up vertical plane, indicated by a small bubble level that should be
for each extrusion plastometer in the laboratory. A replacement placed on the top of the barrel or on the top of the piston when
standard should be introduced before the old standard runs out placed in the barrel. The level should be checked on a regular
and should be compared to the old standard to ensure that any schedule.
shifts seen in the SQC chart are due to the material and not to X2.2.2 Die Orifice Diameter—An undersized die orifice
the equipment. (which can result from a buildup of residue) will cause low
X2.1.1.3 Proficiency Tests—Participation in proficiency test results. Conversely, an oversized orifice (which can result from
programs is important for demonstrating how the laboratory’s wear) will cause high results. It is important that the die orifice
results compare with other laboratories. Over a period of time, be cleaned after each test and that the die orifice diameter be
laboratory bias can be demonstrated, if bias exists. verified frequently using a calibrated go/no-go gauge.
X2.1.1.4 ASTM Round Robins (Interlaboratory Tests)— Remember, the calibrated pin gauge can also wear and the
These programs are similar to proficiency test programs but are diameter should be verified regularly.
limited to only a few laboratories and a few materials. X2.2.3 Die Cleanliness—The die should be completely
However, these programs do provide information on how well cleaned after each test. Any residue left in the orifice will
the laboratory performs the test. eventually char and be very difficult, if not impossible, to
X2.1.1.5 Calibration, Verification, and Maintenance—The clean. Buildup of material will reduce the diameter of the die
extrusion plastometer should be calibrated. Proper mainte- and change the surface smoothness, resulting in erroneous
nance of the instrument will help to ensure proper calibration. results.
(1) As a first step to obtaining reproducible results, opera-
tors should be well trained. Using internal standards can X2.2.4 Temperature in the Barrel—Melt flow rates are very
demonstrate that repeatable results can be provided. The dependent on temperature. The temperature within the barrel is
operators should also understand the test and know what can the only important temperature. Temperature indicators must
affect the results. be calibrated to the temperature within the barrel. High flow
(2) Before starting the test, the following should be veri- rates will result from high temperatures and low flow rates
fied: from low temperatures. Defective heaters may be difficult to
(a) The protocol is understood by the operator. detect and can cause variable results.
(b) The barrel, piston, and die orifice have been properly X2.2.5 Preheat Time—Proper preheat time is required to
cleaned. allow the material in the barrel to fully melt and to come to
(c) The extrusion plastometer, including the piston and temperature equilibrium throughout the barrel. If material is
die, are at equilibrium at the proper temperature. not fully melted, die plugging and low melt flow rates can
(d) The extrusion plastometer is level. result. If not at temperature equilibrium, the melt flow rate will
(e) A standard has been run and the results fall within change as the test is conducted.
established parameters. X2.2.5.1 It is important that the die and piston be at
(3) When a problem arises, the following questions should temperature equilibrium with the rest of the system before any
be asked: sample is introduced into the barrel. If the piston and die are
(a) Did anything unusual happen? not at temperature, the large mass of metal involved must be
(b) Does the extrudate contain air bubbles? heated to temperature during testing and the energy required
(c) Were the proper weights applied? may not allow the polymer to reach thermal equilibrium. This
(d) Is the unit at the proper temperature? can result in erroneous data.
(e) Was the piston stored in the barrel? X2.2.6 Barrel Condition—The barrel should be properly
(f) Is the die damaged, that is, chipped? cleaned after each test. Failure to do so can result in contami-
(g) Is the die bore worn, that is, the diameter is larger than nation of the next sample, and buildup and degradation of
the maximum specified? material in the barrel, resulting in a decrease in the diameter of
(h) Was the proper amount of material used? the barrel. This can cause friction with the piston tip resulting
(i) Has the balance been properly calibrated? in low melt flow rates.
(j) Was the proper purge time used? X2.2.6.1 Frequently overlooked is the condition of the
(k) Was the plug pulled at the proper time? barrel itself. In addition to being clean, the barrel wall must be
(l) Was the correct warm-up time used? smooth and of the proper diameter. The inside diameter of the
(m) Was the barrel cleaned properly? barrel is as important as the diameter of the die orifice. The
(n) Is the piston rod straight? barrel diameter should be measured regularly, and changed if
(o) Is the piston tip diameter OK? so indicated. The melt flow rate is a function of the fourth
power of the barrel diameter.
X2.2 Understanding How Melt Flow Rate is Affected
X2.2.7 Piston Parameters—The diameter of the piston foot
X2.2.1 Levelness of the Instrument—The piston must be should be checked. If it is worn, material can flow back past the
free to move in a vertical position. If the instrument is not level, tip. This would result in erroneous data.
the piston can be slowed by friction as it touches the side of the X2.2.7.1 The piston tip, or foot, is sometimes screwed into
barrel. This will not only introduce an error into the results but the end of the piston and can be changed easily. However,

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D1238 − 13
because it is easily unscrewed, it can work itself loose. The results and a longer than target cut time will give high results.
piston tip must be checked frequently and kept tightly screwed The timing intervals should be verified with certified timers.
into the piston. When cut, the extrudate end should not be ragged or stringy.
X2.2.7.2 Care must be taken not to bend a piston. Even a These variables, if not controlled, can cause poor reproducibil-
slight, almost non-detectable curvature in the piston can result ity of test results.
in the force not being applied directly to the vertical position,
X2.2.13 Purging—Purging the barrel between runs or when
resulting in excessive pressure on the wall of the barrel. This
changing materials is sometimes necessary. Purging with the
will cause low results and can also scratch the barrel wall.
same material which will be tested after the purge is best.
X2.2.7.3 The piston has two reference marks. The lower
However, if for some reason another purge material is used, run
scribe mark on the piston must be at the reference start position
the test material through the barrel before the actual test run in
(top of the guide ring or barrel) at 7.0 6 0.5 min, as stated in
order to ensure that the purge material is no longer in the barrel.
9.8 and 10.9. Starting each test at a different position can give
variable results. X2.2.13.1 Purging does not replace cleaning. After purging,
the equipment must be cleaned properly to avoid the effects of
X2.2.8 Sample Mass—Small variations in sample mass can contamination, resin buildup, and so forth, as discussed previ-
cause significant variability in melt flow rates. Any balance ously.
used to weigh the sample should be calibrated and verified on
a regular schedule. X2.2.14 Melt Density—It is important that the correct melt
density be used, that is, 0.7636 g/cm3 for PE at 190°C and
X2.2.9 Moisture in Sample—Samples should be dried be-
0.7386 g/cm3 for PP at 230°C. These values may be different
fore testing. Some materials may be affected more than others
for copolymers or when additives are incorporated into the
by moisture. However, the presence of moisture during the test,
resin. Small errors in these values can affect the end results. If
in general, will affect the melt flow rates of most materials.
not known, the melt density can be determined as described at
X2.2.10 Sample Purge Time—Purging material from the the end of Footnote A of Table 2.
barrel before the actual test starts serves two primary functions:
(1) to expel entrapped air or volatiles before applying the full X2.2.15 Piston (Flag) Travel Distance—The setting of the
test load, and (2) to move the lower scribe mark on the piston proper piston travel distance (6.35 6 0.25 mm for MFRs up to
to the reference start position. For flow rate consistency, it is 10 g/10 min and 25.40 6 0.25 mm for MFRs greater than 10
important that the extrudate be free of voids and that the test g/10 min) is important in Procedure B. The reproducibility of
always starts with the piston in the same position in the barrel. Procedure B is better if these parameters are strictly adhered to.
Whether in the extrudate for Procedure A or in the barrel for A calibrated distance verification device will be required to
Procedure B, voids will affect test results. maintain the proper piston travel.
X2.2.11 Load Weight—The actual weight (load) applied to X2.2.16 Calculation Factors—When trouble shooting, al-
the material during the test will affect the test results. Higher ways check the calculations and the factors used.
weights will produce higher results. The load weight, which X2.2.17 Power (Electrical) Fluctuation—Constant power
includes the piston weight, should be verified at regular (voltage) is important to maintain the temperature desired.
intervals. Periodic changes in voltage will cause changes in the tempera-
X2.2.12 Extrudate Cut Technique—It is important that good ture of the unit, creating test values that fluctuate because of
extrudate cutting technique be developed. A sharp, clean tool inconsistent sample temperatures. Though this is a rare
should always be used for this operation. The timing of the cut situation, this fluctuation has been found to cause erratic test
is critical since a shorter than target cut time will produce low results.

X3. EXTRUSION PLASTOMETER TEMPERATURE CALIBRATION DEVICE

X3.1 The RTD shall be inserted into a bronze tip. Tip of the depth is 11.2 mm. Clearance between the RTD and the bronze
RTD element shall touch the bronze tip. Minimum insertion tip wall shall be minimized. (See Fig. X3.1.)

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D1238 − 13

FIG. X3.1 Example of a Temperature Calibration Device

X4. SUGGESTED TEST CONDITIONS FOR SELECT MATERIALS

X4.1 Table X4.1 shows a list of common test conditions plastic materials.
used for determining the rate of extrusion for some thermo-

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D1238 − 13
TABLE X4.1 Suggested Test Conditions for Select Materials
Material Temperatures Weights
Acetals (copolymer and homopolymer) 190 1.05
190 2.16
Acrylics 230 1.2
230 3.8
Acrylonitrile-butadienestyrene 200 5.0
220 10
230 3.8
Acrylonitrile/butadiene/styrene/polycarbonate blends 230 3.8
250 1.2
265 3.8
265 5.0
Cellulose esters 190 0.325
190 2.16
190 21.6
210 2.16
Ethylenechlorotrifluoroethylene copolymer 271.5 2.16
271.5 5.0
Ethylene-tetrafluoroethylene copolymer 297 5.0
Polyamide 235 1.0
235 2.16
235 5.0
275 0.325
275 5.0
Perfluoro(ethylenepropylene) copolymer 372 2.16
Perfluoroalkoxyalkane 372 5.0
Polycaprolactone 80 2.16
125 2.16
Polychlorotrifluorethylene 265 12.5
Polyetheretherketone (PEEK) 400 2.16
Polyether sulfone (PESU) 360 10
380 2.16
Polyethylene 125 0.325
125 2.16
190 0.325
190 2.16
190 5
190 10
190 21.6
250 1.2
310 12.5
Polycarbonate 300 1.2
Polymonochlorotrifluoroethylene 265 21.6
265 31.6
Polypropylene 230 2.16
Polyphenyl sulfone (PPSU) 365 5.0
380 2.16
Polystyrene 190 5.0
200 5.0
230 1.2
230 3.8
Polysulfone (PSU) 343 2.16
Polyethylene terephthalate (PET) 250 2.16
285 2.16
Poly(vinyl acetal) 150 21.6
Polyvinyl chloride (PVC), rigid compoundA 190 21.6
Poly(vinylidene fluoride) 230 5.0
230 21.6
Poly(phenylene sulfide) 315 5.0
Styrene acrylonitrile 220 10
230 3.8
230 10
Styrenic Thermoplastic Elastomer 190 2.16
200 5.0
Thermoplastic Elastomer-Ether-Ester 190 2.16
220 2.16
230 2.16
240 2.16
250 2.16
Thermoplastic elastomers (TEO) 230 2.16
Vinylidene fluoride copolymersB 120 5.0
120 21.6
230 2.16
230 5.0
A
Data has shown that greater repeatability and reproducibility when testing PVC can be obtained using Test Method D3364.
B
Tm = 100°C

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D1238 − 13

REFERENCES

(1) “Polyethylene Insulation and Sheathing for Electrical Cables,” Gov- (4) Harban, A. A., and McClamery, R. M., “Limitations on Measuring
ernment Department Electrical Specification No. 27, Great Britain, Melt Flow Rates of Polyethylene and Ethylene Copolymers by
1950. Extrusion Plastometer ,” Materials Research and Standards, Vol 3,
(2) Tordella, J. P., and Jolly, R. E., “Melt Flow of Polyethylene,” Modern No. 11, 1963, p. 906.
Plastics, Vol 31 , No. 2, 1953, p. 146. (5) Rudin, A., and Schreiber, H. P., “Factors in Melt Indexing of
(3) Dexter, F. D., “ Plasticity Grading of Fluorothenes,” Modern Plastics, Polyolefins,” SPE Journal, Vol 20, No. 6, 1964, p. 533.
Vol 30 , No. 8, 1953, p. 125.

SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue, D1238 - 10,
that may impact the use of this standard. (August 1, 2013)

(1) Revised Section 8. (2) Added Appendix X4.

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